Search results for "NMR"
showing 10 items of 1575 documents
Investigation into the reaction of (t-BuC5H4)2Nb(η2-Te2)H with CH3Li: Hydride abstraction versus telluride methylation
2007
Abstract The reaction of [ Cp 2 ′ Nb ( Te 2 ) H ] ( 1 ) (Cp′ = t -BuC 5 H 4 ) with CH 3 Li in THF was examined by variable temperature 1 H NMR, ESR and mass spectroscopic means. From these methods it is evident that the diamagnetic compounds [ Cp 2 ′ NbH 2 ( TeCH 3 ) ] ( 2 ) and [ Cp 2 ′ Nb ( Te ) CH 3 ] ( 3 ) as well as the paramagnetic compound [ Cp 2 ′ Nb ( TeCH 3 ) 2 ] ( 4 ) form simultaneously. In the subsequent reaction of the intermediate solution with [Co 2 (CO) 8 ] compound 4 was consumed and the compound [ Cp 2 ′ Nb ( μ - TeCH 3 ) 2 Co(CO) 2 ] ( 5 ) formed in good yield. Complex 5 was characterized by IR and variable temperature 1 H NMR spectroscopies. Electrochemical two-electro…
Determination of phosphorus compounds in plant tissues: from colourimetry to advanced instrumental analytical chemistry
2022
Although the spectrum of effective methods and techniques that allow determination of inorganic or total phosphorus is impressive, more precise analysis of these substances in plant tissues is not a routine or trivial task. The complexity of chemical composition of plant tissues treated as the analytical matrices is thought to be the main cause why there is no one answer, how appropriate phosphorus compounds may be determined qualitatively and quantitatively. Even if more advanced spectrophotometric measurements and classical variants of absorption (FAAS) or emission (ICP-AES/ ICP-OES) spectrometry techniques are used, it is necessary at first to isolate various forms of phosphorus from the…
Anatase nanoparticles boundaries resulting from titanium tetrachloride hydrolysis
2017
An important factor that governs solar energy transformation into electrical or chemical energy, when using nanoparticles-based devices, is the spatial location of traps limiting electron transport. Evidences have been presented indicating that the electron diffusion is strongly influenced by nanoparticle boundaries, whose characteristics depend on the particles preparation. In the present work we have studied the role of hydrated excess proton structures in the formation of anatase nanoparticles boundaries in samples prepared by TiCl4 hydrolysis at low temperature and strong acidic conditions. The samples, constituted by anatase nanocrystals but, mainly, by amorphous titania, are studied b…
Thermo-responsive hydrogels from cellulose-based polyelectrolytes and catanionic vesicles for biomedical application.
2016
In this study, negatively charged catanionic vesicles/hydrophobically modified hydroxyethylcellulose polymers thermo-responsive hydrogels have been fabricated. Vesicular aggregates were found to act as multifunctional junctions for networking of modified-cellulose water solutions. The contributions of the electrostatic and hydrophobic interactions were evaluated by changing either vesicles composition or the polymer hydrophobic substitution. Thermal-induced size and lamellarity of hydrogel-enclosed vesicles were detected, with further polygonal shape changes induced by cellulose-based polymer addition. The thermal transition was also found to tune hydrogel mechanical behaviour. The network …
Anion Recognition by a Bioactive Diureidodecalin Anionophore: Solid-State, Solution, and Computational Studies
2018
Recent work has identified a bis-(p-nitrophenyl)ureidodecalin anion carrier as a promising candidate for biomedical applications, showing good activity for chloride transport in cells yet almost no cytotoxicity. To underpin further development of this and related compounds, a detailed structural and binding investigation is reported. Crystal structures of the transporter as five solvates confirm the diaxial positioning of urea groups while revealing a degree of conformational flexibility. Structures of complexes with Cl−, Br−, NO3 −, SO4 2− and AcO−, supported by computational studies, show how the binding site can adapt to accommodate these anions. 1H NMR binding studies revealed exception…
Tin(IV) catalyzed D-galacturonic acid anomerization
2008
A comparative kinetic study of anomerization between the four main forms (alpha/beta-pyranosides and alpha/beta-furanosides) of D-galacturonic acid (GalAH(2), 1) and tin(IV) complexed D-galacturonate ([Sn(CH(3))(2)(GalA)(H(2)O)(2)], 2) in D(2)O, is reported. Important differences are shown by pD vs. mutarotation rate profiles of 1 and 2. Coordination, in fact, causes: i) a spectacular increase of the rate due to kinetic template assistance of the carboxylic tail holding the metal in close proximity to the reactive centre and ii) a change in the dependence of the rate on the pD. Entropic and enthalpic factors contribute to the huge activation energy decrease in 2. Anomerization rates of the …
Synthesis, characterization and the first crystal structure of the Zn(II) complex of 4,6-O-ethylidine-N-(2-hydroxybenzylidene)-β-D-glucopyranosylamine
2001
4,6-O-Ethylidine-N-(2-hydroxybenzylidene)-β-D-glucopyranosylamine (H3L1) and N-(5-bromo-2-hydroxybenzylidene-4,6-O-ethylidine-β-D-glucopyranosylamine (H3L2) molecules possessing a–C-1–N=C(H)–moiety for metal-ion binding were synthesized by condensing the 4,6–O–ethylidene–β–D–glucopyranosylamine with salicylaldehyde or 5–bromosalicylaldehyde. Complexes of these ligands with Zn(II) were isolated and characterized using elemental analysis, FTIR, UV–Vis absorption, NMR spectroscopic and FAB mass spectrometric techniques. The structure of the Zn(II) complex derived from H3L1 was established for the first time by a single-crystal X-ray diffraction study. The anomeric nature of the saccharide moie…
Ion-Pairing Effects in the Self-Assembly of a Fluorescent Pseudorotaxane
2006
Herein we report on the self-assembly, in a low polarity solvent, of a pseudorotaxane species comprising binaphthyl-26-crown-8 (BN26C8) as the macrocyclic host and anthracenyl-benzylammonium as the threadlike positively charged guest (ABH+). Absorption and luminescence data reveal a very efficient energy transfer process occurring from the binaphthyl to the anthracene singlet excited states. The self-assembly is highly dependent on the nature of the counteranion confirming the crucial role played by it in the competition between the self-assembly process and the formation of ion pairs (ABH+X-). This behavior can be readily evidenced in dilute solutions from the analysis of the luminescence …
Anti-cancer activity of di- and tri-organotin(IV) compounds with D-(+)-Galacturonic acid on human tumor cells
2018
Abstract We have compared the anti-proliferative activity in vitro, of R2SnGala (1-3) [R = Me, n-Bu, Ph] and novel R3SnGala (4, 5) [R = Me, n-Bu] with D-(+)-Galacturonic acid [HGala; Galaq-, q = (2) and (1) for R2SnGala and R3SnGala, respectively] compounds, towards human tumor cell lines of intestinal carcinoma (HCT-116) and breast adenocarcinoma (MCF-7). The new synthesized 4 and 5 compounds were characterized, in solution, by 1H, 13C and 119Sn NMR, that showed that HGala acts as monoanionic moiety and evidenced the dynamic behavior of the compounds, due to inter-conversions involving the anomeric carbon atom of the ligand. Cell viability, apoptosis induction and cell cycle distribution w…
Correlation spectroscopy in molten and supercooled antimony trichloride.
1990
Correlation spectroscopy measurements performed on molten and supercooled antimony trichloride with the homodyne technique show correlation functions that have a nonexponential behavior. Two well-defined distributions of correlation times can be observed in different temporal regions. This behavior is discussed in terms of a structural relaxation of clusters dynamically formed by intermolecular and interchain bonds. The Arrhenius plot of these correlation times shows a linear behavior with the same activation energy for both. In contrast, the activation energy of shear viscosity has a different value, showing that the processes determining the temperature behavior of \ensuremath{\tau} and $…